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Water → 3-Methyl-1-(4-methylphenyl)butan-1-one

HRID 1190945
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HRID 1190945 반응식
[Cl-].[Cl-].[Cl-].[Al+3].[C:5](Cl)(=[O:10])[CH2:6][CH:7]([CH3:9])[CH3:8].O.[C:13]1([CH3:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>>[CH3:8][CH:7]([CH3:9])[CH2:6][C:5]([C:16]1[CH:17]=[CH:18][C:13]([CH3:19])=[CH:14][CH:15]=1)=[O:10]
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참가 물질

5

반응물 4

HCID 962WaterHCID 1140TolueneHCID 66054Isovaleryl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 125064723-Methyl-1-(4-methylphenyl)butan-1-one수율 97%

실험 절차

Portionwise add aluminum trichloride (3.35 g, 25 mmol) to a solution of isovaleryl chloride (2 mL, 16.4 mmol) in anhydrous toluene (50 mL) at 0° C. Warm to room temperature and stir 12 h. Cool to 0° C. and slowly add cold water (500 mL). Extract with EtOAc, wash the organic phase with brine, dry over Na2SO4 and concentrate in vacuo to obtain the desired intermediate (2.8 g, 97%) as an orange oil suitable for use without additional purification. MS (APCI+) m/z: 176 (M+).

후처리

  1. customat 0° C
  2. temperatureCool to 0° C.
  3. extractionExtract with EtOAc
  4. washwash the organic phase with brine
  5. dry with materialdry over Na2SO4
  6. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-79bb30e5a361426bb5134cb3c562e4c0
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680091B2

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